DE GRUYTER Physical Sciences Reviews.

2020; 20190083

Adrianna Nogalska1,2,3 / Anna Trojanowska1,3 / Bartosz Tylkowski1,2 / Ricard Garcia-Valls1,2,3

Surface characterization by optical contact

angle measuring system
1 Centre Tecnològic de la Química de Catalunya (CTQC), Tarragona, Spain, E-mail: [email protected],

[email protected], [email protected], [email protected]

2 Eurecat Centre Tecnològic de Catalunya, Tarragona, Catalunya, Spain, E-mail: [email protected],

[email protected], [email protected]
3 Departamento de ingeniería química, Universitat Rovira i Virgili, Av. dels Països Catalans 26, Tarragona 43007, Spain, E-mail:

[email protected], [email protected], [email protected]

Abstract:
Constant development of novel materials and their characterization is a highly important matter nowadays. Op-
tical contact angle measuring system is a very versatile tool among the surface characterization techniques. The
main application of the technique is determination of hydrophobicity/hydrophilicity and wetting properties
of materials. Current generation machines are fully automatized with a number of complements for temper-
ature and pressure control, nanoliter drop generation, etc. Besides commenting on the current state of the art
of the equipment, their capabilities and costs, this review includes some practical tips on the execution of the
technique and data analysis.
Keywords: contact angle, wetting, surface characterization, hydrophobicity, hydrophilicity
DOI: 10.1515/psr-2019-0083

1 Introduction
Material surface properties are very important for its final use especially when it comes to protective coating,
surface activation by bonding or its general modification. The influences of the treatments can be analyzed and
optimized thanks to contact angle measuring systems, among others.
The contact angle is an angle formed between a liquid and a solid surface which results from liquid/solid/-
gas phase interfacial tensions. Thanks to contact angle measurements it is possible to analyze how a material
is wetted by a liquid: the smaller is the contact angle value the higher will be wettability.
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An increase of the interest in surface characterization by optical contact angle measuring system over the
years is highlighted by statistical analysis: an analysis by Scopus (TITLE-ABS-KEY: optical AND contact AND
angle AND measurement) shows that since 1941 there are 2506 documents published on the subject. A real
increase of the amount of publications falls on the 1987 year according to the chart on Figure 1(a). The technique
is used in a great number of scientific areas (Figure 1(b)), and mainly in: Materials Science (1424 documents),
Physics and Astronomy (1168 documents), Engineering (1036 documents) and Chemistry (672 documents).

Adrianna Nogalska is the corresponding author.

© 2020 Walter de Gruyter GmbH, Berlin/Boston.

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Figure 1: Statistical data (a) increase of publications in time and (b) documents divided in subject area. (Tool used: Sco-
pus, April 2019).

The aim of the review is to provide the information on the current state of art of surface characterization by
optical contact angle measuring systems. An overview on the machines as well as on the technique and its
performance is included, which can be especially useful for the technicians or the scientists which are looking
for an appropriate apparatus.

2 Theory
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It must be highlighted that the origins and importance of the contact angle date back to the XIX century when
the famous works on cohesion and adhesion of fluids have been published by Thomas Young and Athanase
Dupré [1]. Young [2] in 1805 defined the contact angle, when he was analyzing the adhesion of a liquid to a
solid, in a three phase system (Figure 2). According to the Young theory the contact angle (θY ) and the surface
tension (σ) of each phase component are mathematically related by the following equation derived by Dupre
in [3]:

𝜎𝑆𝐺 − 𝜎𝑆𝐿
cos 𝜃𝑌 = (1)
𝜎𝐿𝐺

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Figure 2: Contact angle.

where σSG , σSL , σLG represent the interfacial tension of respectively solid/gas, solid/liquid, liquid/gas inter-
phases. However, the equation is only applicable for systems containing ideal surfaces in terms of homogeneity,
smoothness and rigidness. For this reason, Athanase Dupré in 1869 considered the work of adhesion (𝑊𝑠𝐿 ) for
two immiscible liquids in contact. Thus, according to Dupré, the work done on separating a phase S from a
phase L across the surface of separation is defined as:

𝑊𝑠𝐿 = 𝜎𝑠𝑣 + 𝜎𝐿 − 𝜎𝑠𝑙 (2)

Finally, the work of adhesion could be calculated by combination of both scientists’ achievements in the Young–
Dupré equation:

𝑊𝑠𝑙 = 𝜎𝐿 (1 + cos 𝜃𝑌 ) (3)

According to the “old school terminology” the surface tension phenomenon is explained through the example
of the water droplet shape (Figure 3): in a water droplet bulk, the molecules are pulled equally in every direction
by the other molecules in their vicinity, and this leads to a null net force; on the other hand for the surface
molecules the net force pulls inward, as they are not entirely surrounded by other water molecules. This way
an internal pressure is created, forcing the surface to contract to minimize the droplet surface area, configuration
that corresponds to the shape of a sphere.

Figure 3: Surface tension of water droplets. The blue spheres represent water molecules and black arrows direction of the
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cohesive forces.

However, following the recently published articles [4], the origin of surface tension is related to the unusual
energetic state of the surface molecule, which misses half its interactions. The energy states of molecules in the
bulk and at the surface of liquid are not the same due to the difference in the nearest surrounding of a given
molecule. Each molecule in the bulk is surrounded by others on every side, whereas, for the molecule located at
the liquid/vapor interface, there are very few molecules outside. Obviously, the net force acting on a molecule
in equilibrium is zero.
It is worth mentioning that the droplet molecules are in constant movement, with new water molecules
brought to the surface in contact with the gas phase all the time. This means that the droplet has more than one
thermodynamic equilibrium state. Thus for a proper analysis of the wetting it has to be taken into account the
contact angle hysteresis which θh is measured by means of dynamic contact angle. In this measurement, the
droplet is in motion by being expanded and constrain through adding and withdrawing a liquid volume with a
needle. The hysteresis (eq. 4) is defined as difference between advancing θa and receding θr contact angle, with
the advancing one being the maximum and the receding one being the minimum contact angle. On an ideal
surface the hysteresis is equal 0, but in practice its value increases with increase of the surface roughness and
heterogeneity:

𝜃ℎ = 𝜃 𝑎 − 𝜃 𝑟 (4)

As mentioned before, the Young equation is used for perfectly smooth and homogenous surfaces. However,
surfaces in real samples behave differently than ideal ones, thus the application of Young equation is not rec-
ommended as it might give incorrect results. The influence of the surface roughness on the resulting contact
angle was firstly analyzed by Wenzel [5] in 1936 and further by Cassie [6] in 1944.

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According to Wenzel model, when the droplet is placed on a rough surface, the contact surface area between
the liquid and the solid increases. In the Wenzel model water is assumed to be completely in contact with surface
(Figure 4). The contact angle equation was modified with a roughness ratio factor (r), which is defined as the
ratio of the real area to its projection:

cos 𝜃𝑊 = 𝑟𝑐𝑜𝑠𝜃𝑌 (5)

Figure 4: Contact angle modules by Young, Wenzel and Cassie-Baxter. Half spheres represent water droplets, black lines
contacting surface of grey material.

According to this model, the surface roughness enhances the surface properties. In other words, hydrophobic
surface became more hydrophobic whereas hydrophilic ones became more hydrophilic.
The Cassie-Baxter model describes a situation in which when the drop is placed on a heterogeneous ma-
terial more than one factor is included in the final surface roughness. The model gives an explanation to the
“lotus effect”: when a droplet is placed on a highly hydrophobic and rough surface, it distributes on the solid
roughness’ peaks and on the so-called air-pockets (Figure 4). In this case the energy of a partial contact with
the solid surface is much smaller comparing to the energy of complete contact as in case of hydrophilic surface
in Wenzel‘s model. Here, the contact angle equation for composite material surface is the following:

cos 𝜃𝐶𝐵 = 𝑟𝑓 𝑓 𝑐𝑜𝑠𝜃𝑌 + (𝑓 − 1) (6)

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where rf is the wet surface area roughness ratio, while f is the fraction of the wet surface area.

3 Sample preparation
During the sample preparation, contamination must be avoided for both the analyzed surface and the liquid
used for it. If the surface is polluted with lipids or salts from the user’s hands, it may have an influence on the
surface’s final contact angle, while the presence of particles in the liquid changes its density and, again, the
contact angle would be affected by it. Moreover, in order to obtain a reliable and repetitive value, the sample
surface must be chemically and physically homogeneous. At the same time, no chemical reaction between the
drop and the material must occur, thus they must be compatible.
Besides the aforementioned precautions, the sample preparation is a rather simple process. Basically, the
sample must be placed on a support in the corresponding position, depending on the equipment, with the
surface of interest facing the needle.

4 Current generation machines

The current generation machines are fully automatized, from the drop creation to contact angle calculation for
both static and dynamic measurements. Moreover, it is possible to not only to take an image but to record a live
video of the analyses. Novel equipment allows you to perform measurements in a controlled atmosphere and
to measure the contact angle of other liquids than water. The machines make use of a light that does not heat up

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the sample and therefore does not cause evaporation: warm light LED with variable intensity control ensures
extreme low heat radiation. Machines can be found from portable units, to ones with multi-liquid dispensers
to ones that can control temperature.
Recently, it was found that the control of the analysis conditions such as temperature, pressure or gas phase
composition plays and important role in understanding the wetting. In order to meet the requirement of cus-
tomers, producers build additional accessories in the form of chambers which can be implemented to the stan-
dard device. Thus there is no need of buying a new device. The chambers allow temperature control up to
200 °C, and pressure control up to 400 bars. This is mainly applied in enhanced oil recovery and supercritical
fluid analysis. Furthermore, the gas tight chamber can be filled with oxidizing, reducing or inert gas, and even
vacuumed.
Besides, a novel device uses a drop-shape analysis to characterize surface/drop interactions in metallurgy,
where melts meet solid surface. It can work in very high temperature, even up to 2000 °C and in various atmo-
spheric conditions, which allows to simulate industrial processes and to optimize them.
Kruss came up with a solution for contact angle measurements of surfaces with depressions, for which the
conventional side view cannot be applied. The instrument (Figure 5) analyzes the drop shape from above using
the top-view reflection method. Here, the contact angle is measured based on the distance of light spots which
are reflected at the surface of the drop.
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Figure 5: Top view analyzer – TVA100. (Reprinted with permission from Instrumentación Analítica S.A.).

Portable devices (Figure 6) are a good solution for measurements on hard-to-reach surfaces (horizontal, verti-
cal, inverted, blind, contoured, and textured), especially out of laboratories or when it is not possible collect a
sample. This type of devices needs to be light and have long lasting batteries. Dyne testing offers equipment
that works with HPLC water, weight only 0.5 kg and can operate for 5 h. Moreover it contains a Video Scope
for in-situ analysis.

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Figure 6: Portable device from Dyne testing. (Reprinted with permission from Lasing S.A.).

As for measuring of dynamic contact angles by a tilting method, the solid sample has to be tilted from its
horizontal position. The new generation machines are often complemented with substrate holder which can
bend up to 180°.
Another challenge in the optical contact angle measuring systems is the microstructures’ surface charac-
terization for samples such as small medical products, precision mechanics or wires and fibers. The standard
size of a created drop is in microliter size range; however, a novel dosing system capable to create a 100 times
smaller drop has been developed. This is made possible by a nanoliter dosing vale, which uses an air-filled sy-
ringe and triggers magnetic forces. The nanoliter drop created on a dental implant screw is presented in Figure
7.
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Figure 7: Dosing systems for microstructures. (Reprinted with permission from DataPhysics Instruments GmbH).

Besides improving the machines, scientists are also making advances in the software area. An interesting feature
was implemented by Attension with the surface roughness being automatically corrected for the contact angle
measurements results. The method principles are illustrated on Figure 8. Surface roughness measured with
the module is based on structured lighting, where the light is projected on surface and the camera is capable
to reconstruct it in 3D. After that it uses the Wenzel theory for calculating corrected contact angle values.

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Figure 8: 3D Topography module roughness-corrected contact angle measurements. (Reprinted with permission from
Lasing S.A.).

5 Capabilities
The usual measuring range of contact angle measuring systems is 0–180°. The novel machines are very precise
with accuracy varying between ±0.1–0.3° and resolution of around ±0.1°. Moreover the sample size that can be
place on the equipment is very large (3–10 kg) and in case of portable equipment the size does not matter.
This kind of surface characterization technique found useful applications not only in scientific world but
also in everyday life products development. It is a useful tool for determining the biocompatibility of medical
implants such as bone or dental prostheses (Figure 9). The surfaces exhibiting a high surface free energy were
found to be the best material for the application. For this reason hydrophobic materials are frequently modified
for surface activation. Thus contact angle measuring systems allow to follow the modification progress. Jemat
in her thesis [7] describes the wettability improvement of the dental implant surface made of titanium. This was
achieved by chemical treatments using acidic or alkali titanium alloys. The treatment leads to improvement of
cell/implant adhesion and accelerate curing process.
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Figure 9: Dental prosthesis with titanium screws.

Another application can be found in hair care products developments, where the hair wettability plays an
important role (Figure 10). The cosmetics are specifically produced for different hair types and always leave
their surface changed. Novel machines are capable to measure the contact angle of a single hair. Trybala et al.
[8] studied the influence of a polyacrylate polymer on dry hair wetting. A dry and undamaged hair is typically
hydrophobic, thus a selection of proper polymer solution is crucial for the hair treatment in order to achieve its
fast or slow penetration into the hair depending on the application. The contact angle measuring system allows
to follow the influences of each component of the polymer-containing solution on hair wetting.

Figure 10: Water drop on human hair.

The measurements of the surface tension and contact angle are very helpful for optimizing the production of
paints or other kinds of coatings, especially when they are to be used on wood. Different kinds of wood require
different coatings with different properties, but the most important one is good adhesion and proper bonding
to the surface. In general there is a good correlation between contact angle and penetration [9]. The coating
must have lower surface free energy (30–40 mJ m−2 ) than wood (40–50 mJ m−2 ) in order to wet it.
For purely scientific applications, the optical contact angle measuring system is mainly use for the charac-
terization of developed new materials or for the improvement of existing materials by modifications. Rezaei
et al. [10] created a coating which is both hydrophobic and lipophobic. The coating consists of polymers mixed
with silica nanoparticles and the polymer precursors are made of a ternary thiol-epoxy-acrylate mixture. For
the analysis of the coating influence on the modified surface properties, the authors performed the contact an-
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gle measurements of water, n-dodecane (oil) and diiodomethane in order to obtain data for the hydrophobicity
and lipophobicity. Superhydrophobic and lipophobic properties were only achievable by adding MSiNP to the
coating.
The technique can be used also to prove that modifications applied have been done properly. For example,
Hiroki Nagasawa et al. [11] in their studies coated the UV degradable plastic of PMMA with TiO2 . The contact
angle of the treated surface decreased from 73° to 29°, demonstrating that the formation of a thin TiO2 layer on
top of the polymeric film was done. Mohor’s group [12] used it not only to follow the modification process but
also to investigate use of different solvents on produced coating properties. The coating was prepared to be used
for bronze art protection in a removable way. It was made of resins and copolymers. Studies showed that the use
of organic solvents for the coating production result in higher contact angle (106°), and more effective protection
comparing to the one obtained with use of water (79°). Studies reveled how different the characteristics of
fluoropolymer resins one can obtain by only changing the solvent used for the preparation.
Coppola et al. [13] studied the influence of the change of experimental conditions on the contact angle of a
surface. The conducted studies had the objective of investigating the influence of 3D printing temperature on
the contact angle, among others. They were able to prove that the higher is the printing temperature, the more
hydrophilic will be the obtained specimen surface. Moreover, they noticed that introduction of nanoparticles
results in lower contact angle comparing to pristine material.

6 Costs
The price range of the optical contact angle measuring systems is very wide and it depends on the brand,
equipment specifications in terms of automatization and accessories.

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Dataphysics has a very large offer of the systems and their prices vary in 10,000–80,000€. Kruss sells auto-
matic apparatus with a price starting from 14,000 to 36,000€. The most expensive one includes fully software
controlled device which can use up to 8 different liquids and can be used for contact angle, surface free energy
of solids and interface and surface tension of liquids measurements.
Another brand, Attensions, offers very competitive prices which starts already from 8700€. Moreover in this
case the cost includes a computer, its installation and training on both the equipment and software.
However, the cheapest models can be purchased in India. Although Holmarc has only 3 models of contact
angle meters in the offer, the most expansive one includes temperature control, rotatable substrate holder and
automated dispenser cost only 6000US$, but the price is not including computer.

7 Companies and brands

The global market leader in the field of surface tension and interfacial tension measurement is the German brand
Kruss. In their wide products offer one can find tensiometers, drop shape analyzer and foam analyzers, which
can work also at a high pressure or temperature, as well as software for the data analysis called ADVANCED.
Kruss is collaborating with many well-known companies such as Airbus, EXXON, Mercedes, Siemens, Apple,
Samsung, BASF, Nestlé, L’Oréal and many others. Moreover, in 2018 the company was included for the third
time in Top 100 Innovators of the German market.
DataPhysics Instruments is also a German company, which has been on the market for 20 years. Besides the
optical contact angle measuring systems, in static and dynamic modes, they provide spinning drop tensiome-
ters and analysis systems for liquid dispersions. What is more important is that the company not only offer the
products, such as devices and software, but they also offer samples analysis or even access to the center if the
samples require an analysis which is not available for the customer.
Biolin Scientific is a leading Nordic instrumentation company with roots in Sweden and Finland. In the com-
pany portfolio we can find brand called Attension, which focuses on general surface measurement technology,
surface energy and surface tension, adhesion and gloss level producing fully automatized optical tensiometers.
They are cooperating mainly with universities.
In India, Holmarc Opto-Mechatronics (P) Ltd. manufactures a variety of scientific and engineering instru-
ments for research, industry and education, and among them is the optical contact angle measuring system.
The additional products they provide are standards for the liquid characterization made of aluminum, brass
and stainless steel. Nonetheless, substrates of the costumers need can also be loaded into the equipment. An-
other interesting feature of their equipment is that the surface over which contact angle is to be measured can
be rotated at ±180 degree from its horizontal position, which is very useful for advanced contact angle study
and to obtain contact angle hysteresis.
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8 Practical information – “how to perform the technique”

Before starting measurements it has to be sure whether the solvent and solid material are adequate for the
characterization or not and that they are compatible with each other, i. e. that they do not react or that the solid
material is not soluble in the liquid. The hydrophilicity/hydrophobicity determination must be performed
with milli-q or deionized water as reference liquid. Selection of the appropriate experimental conditions is
very important and directly dependent on the materials to be characterized and their final applications. For
example materials which are easily undergoing oxidation should be held in inert gas conditions; if the material
to be worked with will be finally supplied to be used in high temperature but it should still remain oil repellent,
one cannot perform measurements in ambient conditions using water as reference liquid.
It is recommended to use a separated syringe for each liquid and always keep them clean. Any contami-
nation of the liquid used for the analysis might results in a change of the liquid properties, such as density,
what would give incorrect information. Moreover, care should be put when filling the syringe to avoid bubbles
formation (Figure 11(b)). Here again, air in the drop can influence the density, the shape, or the volume of the
drop. An air bubble is recognizable in the image as a wide white stripe, which seems to run through the drop.

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Figure 11: Drop formation: (a) correct drop, (b) air in drop, and (c) crawling drop.

Another inconvenience is a drop crawling up on the needle instead of being created under it (Figure 11(c)). This
phenomenon occurs due to electrostatic interactions and can be prevent by applying a hydrophobic substance
on the needle.
The contact angle is measured by software based on the contrast between the drop/surface and the light on
the background, thus the light intensity must be adjusted for the correct definition of the drop shape. Moreover,
it is necessary to adjust properly optics and image in terms of contrast and brightness to obtain the high quality
image.
General practical information:

– Perform 4 or more measurements in different points of the same sample. This can give an idea on homoge-
neously of the material.
– The measuring conditions are always influencing the results, thus one must be sure that all the measurements
are performed in the same conditions, such as drop size and the dosing speed, for achieving reproducibility.
– The same applies for samples preparation: all of the samples must undergo the exact same procedure.

9 Data analysis – “how to interpret the results”

The contact angle is usually used to analyze the hydrophobic/hydrophilic properties of surface, thus the most
commonly used solvent in the analysis is water. The analysis of results obtained for apparent contact angle
measurements (static) is rather simple (Figure 12): a value above 90° indicates a hydrophobic character of the
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surface, while for a value below 90° the surface is considered hydrophilic. In other words, the higher is the value
the more hydrophobic character has analyzed surface. The maximum contact angle is 180° for water-repellent
surfaces and the minimum is 0° for surfaces with very high affinity to water and that get very easily wetted.

Figure 12: Static contact angle micrographs of hydrophilic, hydrophobic and super hydrophobic surfaces: (a) schematic
representation and (b) real life examples.

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Recently, an open discussion on a past mistakes has divided the scientific community as advances made in
the 20th century continue to shaped current interpretations of experimental contact angle [18]. According to
Marmur and co-workers [14] an accurate terminology should be used. The authors suggest that instead of “static
contact angle”, the scientists should use the “apparent contact angle”, because it is the most stable contact angle
and it is the only one that can be routinely measured. In current review we use the term “static contact angle”
only in order to differentiate it from the dynamic one.
According to de Gennes [15] the dynamic contact angle is formed only when the substrate moves, and
it should not be mixed with the advancing and receding contact angles, which are essentially static contact
angles. However in the equipments manuals we can still find references to measure the dynamic contact angle
in terms of advancing and receding one. Advancing and receding measurements (ARCA) (Figure 13), where
the volume of liquid is added and then withdrawn from the drop placed on the analyzed surface, gave us a
plot with the highest and the lowest contact angle value (Figure 14). The maximum corresponds to advancing
contact angle value while the minimum to receding. The difference between advancing and receding value is
called hysteresis and it can give you information about the stability of the droplet/surface interface. The low
value of hysteresis refers to a very small change within the interface where the ideal value for a stable interaction
is 0°, thus the surface wetting is discarded.

Figure 13: Schematic representation of ARCA measurement. Blue half spheres represents water droplets, grey arrows the
needle and direction of liquid flow, while the black arrows expansion and contraction of the droplet.
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Figure 14: ARCA measurements graph with highlighted values corresponding to advancing and receding contact angle
results. (Reprinted from “Operating manual OCA 15EC Video-based optical contact angle measuring instrument” Filder-
stadt, 2013 with permission from DataPhysics Instruments GmbH).

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Another method used for hysteresis determination is tilted plane method. Here again a value of advancing
and receding contact angle is obtained (Figure 15) respectively on the head and back of the droplet. Moreover
this method gives us a value of tilt angle – one more factor used for wetting determination, the angle between
the analyzed surface and table or support at which the drop starts to roll-off. Super hydrophobic surfaces are
characterized by low tilt angle, sometimes even below 10° [16]. The roll-off phenomenon was the base for the
development of self-cleaning surfaces. Rolling drops capable to carry dirt away are very useful for example in
case the of glass surfaces of cars windows. It should be emphasized that the contact angle hysteresis depends
strongly on the method, used for its establishment [17].

Figure 15: Tilted plane method.

10 Summary
The surface characterization technologies have a wide variety of applications not only in strictly scientific fields,
such as new materials preparation and their improvement, but also in costumer goods development. The optical
contact angle measuring system serves for hydrophilic or hydrophobic properties determination. The review
explains the theoretical background behind the technique, the state-of-art of the machines, as well as their cost
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and producers. Moreover, practical information on the sample preparation, measurements performance and
results analysis were included.

11 Conclusions
From the statistical analysis results it was highlighted a rapid increase in the interest within the field and the
wide range of areas using the optical contact angle measuring systems. This led to a fast development of new
machines, which are becoming more and more automatized and precise. The market is dominated by two
leading companies from Germany. The costs are varying from 80,000€ to 6000€ depending on the brand and
specifications. Generally the technique is rather easy to perform and does not require a complicated sample
preparation. Another advantage of the optical contact angle measuring method is the fact that for the analysis
one needs a very small amount of liquid and an accordingly small surface of material. Moreover, the analysis
of obtained data, independently on if it comes to static or dynamic measurements, is simple and gives direct
information about the surface character. On the other hand, the method is relatively sensitive for impurities
and relies on the precision of the operators adjusting the light/brightness/contrast.

Acknowledgements

The authors would like to acknowledge the providers of the contact angle measuring devices for collabora-
tion: Kruss (represented by Instrumentación Analítica S.A.), Holmarc Opto-Mechatronics Pvt Ltd, Dyne testing

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(represented by Lasing), DataPhysics Instruments GmbH. This work is financially supported by Ministerio de
Economía y Competitividad (ENE2017-86711-C3-3-R).

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